RU2017144107A - CATALYSTS BASED ON THE DISINFECTED ZSM-5 FOR ISOMERIZATION OF XYLENE - Google Patents

CATALYSTS BASED ON THE DISINFECTED ZSM-5 FOR ISOMERIZATION OF XYLENE Download PDF

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RU2017144107A
RU2017144107A RU2017144107A RU2017144107A RU2017144107A RU 2017144107 A RU2017144107 A RU 2017144107A RU 2017144107 A RU2017144107 A RU 2017144107A RU 2017144107 A RU2017144107 A RU 2017144107A RU 2017144107 A RU2017144107 A RU 2017144107A
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acid
zsm
zeolite
gram
silica
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RU2017144107A
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RU2724107C2 (en
RU2017144107A3 (en
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Филип НЮБЕЛ
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Бипи Корпорейшен Норт Америка Инк.
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    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
    • B01J29/405—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
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Claims (24)

1. Способ получения катализатора изомеризации ксилола, предусматривающий стадии:1. A method of producing a xylene isomerization catalyst, comprising the steps of: (i) контактирования исходного материала на основе цеолита типа ZSM-5, имеющего мольное отношение диоксида кремния к оксиду алюминия от приблизительно 20 до приблизительно 50 и площадь поверхности мезопор в диапазоне от приблизительно 50 м2/грамм до приблизительно 200 м2/грамм, в реакторе с основанием при температуре от приблизительно 20°С до приблизительно 100°С в течение периода щелочной обработки от приблизительно 1 минуты до приблизительно 10 часов с получением промежуточного цеолитного материала, причем цеолит типа ZSM-5 находится в основании в количестве от приблизительно 1 масс. % до приблизительно 20 масс. %;(i) contacting a ZSM-5 type zeolite source material having a silica to alumina molar ratio of from about 20 to about 50 and a mesopore surface area in the range of from about 50 m 2 / gram to about 200 m 2 / gram, a reactor with a base at a temperature of from about 20 ° C to about 100 ° C for a period of alkaline treatment of from about 1 minute to about 10 hours to obtain an intermediate zeolite material, and the zeolite type ZSM-5 is in the base an amount from about 1 wt. % to about 20 mass. %; (ii) извлечения промежуточного материала на основе цеолита типа ZSM-5 стадии (i);(ii) recovering a ZSM-5 type zeolite intermediate material of step (i); (iii) контактирования промежуточного цеолитного материала с кислотой при температуре от приблизительно 20°С до приблизительно 100°С в течение периода кислотной обработки от приблизительно 1 минуты до приблизительно 10 часов с получением обработанного кислотой продукта на основе цеолита типа ZSM-5;(iii) contacting the intermediate zeolite material with an acid at a temperature of from about 20 ° C to about 100 ° C for an acid treatment period of from about 1 minute to about 10 hours to obtain an acid-treated product based on zeolite type ZSM-5; (iv) извлечения обработанного кислотой продукта на основе цеолита типа ZSM-5 и(iv) recovering an acid-treated product based on zeolite type ZSM-5; and (v) прокаливания обработанного кислотой материала на основе цеолита типа ZSM-5 при температуре в диапазоне от приблизительно 300°С до приблизительно 700°С в течение периода времени в диапазоне от приблизительно 0,2 часа до приблизительно 6 часов с получением продукта на основе обескремненного цеолита типа ZSM-5 с мольным отношением диоксида кремния к оксиду алюминия от приблизительно 20 до приблизительно 150 и с площадью поверхности мезопор в диапазоне от приблизительно 100 м2/грамм до приблизительно 400 м2/грамм.(v) calcining an acid-treated ZSM-5 type zeolite material at a temperature in the range of from about 300 ° C to about 700 ° C for a period of time in the range of from about 0.2 hours to about 6 hours to obtain a silica-free product zeolite type ZSM-5 with a molar ratio of silica to alumina of from about 20 to about 150 and with a mesopore surface area in the range of from about 100 m 2 / gram to about 400 m 2 / gram. 2. Способ по п. 1, в котором исходный материал на основе цеолита типа ZSM-5 имеет среднюю длину, ширину и толщину кристалла менее 1 микрона.2. The method according to p. 1, in which the source material based on zeolite type ZSM-5 has an average length, width and thickness of the crystal of less than 1 micron. 3. Способ по п. 1, в котором основание выбирают из группы, состоящей главным образом из:3. The method according to p. 1, in which the base is selected from the group consisting mainly of: NaOH, LiOH, KOH, RbOH, CsOH, Mg(OH)2, Ca(OH)2, NH4OH, Li2O, Na2O, K2O, Rb2O, Cs2O, MgO и CaO; илиNaOH, LiOH, KOH, RbOH, CsOH, Mg (OH) 2 , Ca (OH) 2 , NH 4 OH, Li 2 O, Na 2 O, K 2 O, Rb 2 O, Cs 2 O, MgO and CaO; or алкоксидов щелочных металлов с формулой R'OM, где R' выбирают из группы, состоящей главным образом из метила, этила, пропила, изопропила, бутила, пентила и фенила, а М выбирают из группы, состоящей главным образом из Li, Na и K; илиalkali metal alkoxides of the formula R'OM, where R 'is selected from the group consisting mainly of methyl, ethyl, propyl, isopropyl, butyl, pentyl and phenyl, and M is selected from the group consisting mainly of Li, Na and K; or гидроксидов алкиламмония с формулой R''NH3OH, R'' 2NH2OH, R'' 3NHOH, R'' 4NOH, где R'' выбирают из группы, состоящей главным образом из метила, этила, пропила, изопропила и, бутила; илиalkylammonium hydroxides of the formula R ″ NH 3 OH, R ″ 2 NH 2 OH, R ″ 3 NHOH, R ″ 4 NOH, where R ″ is selected from the group consisting mainly of methyl, ethyl, propyl, isopropyl and butyl; or любой их комбинации.any combination of them. 4. Способ по п. 3, в котором основание добавляют в реактор порционно во время периода щелочной обработки.4. The method of claim 3, wherein the base is added portionwise to the reactor during the alkaline treatment period. 5. Способ по п. 3, в котором основание добавляют в реактор непрерывно во время периода щелочной обработки.5. The method according to p. 3, in which the base is added to the reactor continuously during the alkaline treatment period. 6. Способ по п. 1, в котором кислоту выбирают из группы, состоящей главным образом из HF, HCl, HBr, HI, HNO2, HNO3, H2SO3, H2SO4, Н3РО3, Н3РО4, Н3ВО3, щавелевой кислоты, лимонной кислоты, уксусной кислоты, бензойной кислоты, муравьиной кислоты, пропионовой кислоты, фторуксусной кислоты, трифторуксусной кислоты, молочной кислоты, виннокаменной кислоты, аскорбиновой кислоты, малоновой кислоты, малеиновой кислоты, янтарной кислоты, глутаровой кислоты, адипиновой кислоты, 2-гидроксибензойной кислоты, 3-гидроксибензойной кислоты и 4-гидроксибензойной кислоты, или любой их комбинации.6. The method according to p. 1, in which the acid is selected from the group consisting mainly of HF, HCl, HBr, HI, HNO 2 , HNO 3 , H 2 SO 3 , H 2 SO 4 , H 3 PO 3 , H 3 PO 4 , H 3 BO 3 , oxalic acid, citric acid, acetic acid, benzoic acid, formic acid, propionic acid, fluoroacetic acid, trifluoroacetic acid, lactic acid, tartaric acid, ascorbic acid, malonic acid, maleic acid, succinic acid, glutaric acid, adipic acid, 2-hydroxybenzoic acid, 3-hydroxybenzoic acid and 4-hydroxybenzoic acid you, or any combination of them. 7. Способ получения катализатора изомеризации ксилола, предусматривающий стадии:7. A method of producing a xylene isomerization catalyst, comprising the steps of: (i) контактирования исходного материала на основе цеолита типа ZSM-5, имеющего мольное отношение диоксида кремния к оксиду алюминия от приблизительно 25 до приблизительно 50 и площадь поверхности мезопор в диапазоне от приблизительно 90 м2/грамм до приблизительно 150 м2/грамм, в реакторе с NaOH при температуре от приблизительно 70°С до приблизительно 90°С в течение периода щелочной обработки от приблизительно 30 минут до приблизительно 120 минут с получением промежуточного цеолитного материала;(i) contacting a ZSM-5 type zeolite source material having a silica to alumina molar ratio of from about 25 to about 50 and a mesopore surface area in the range of from about 90 m 2 / gram to about 150 m 2 / gram, a NaOH reactor at a temperature of from about 70 ° C to about 90 ° C during an alkaline treatment period of from about 30 minutes to about 120 minutes to obtain an intermediate zeolite material; (ii) извлечения промежуточного материала на основе цеолита типа ZSM-5 стадии (i);(ii) recovering a ZSM-5 type zeolite intermediate material of step (i); (iii) контактирования промежуточного цеолитного материала со щавелевой кислотой при температуре от приблизительно 20°С до приблизительно 90°С в течение периода кислотной обработки от приблизительно 60 минут до приблизительно 300 минут с получением обработанного кислотой продукта на основе цеолита типа ZSM-5;(iii) contacting the intermediate zeolite material with oxalic acid at a temperature of from about 20 ° C to about 90 ° C for an acid treatment period of from about 60 minutes to about 300 minutes to obtain an acid-treated ZSM-5 type zeolite product; (iv) извлечения обработанного кислотой продукта на основе цеолита типа ZSM-5 и(iv) recovering an acid-treated product based on zeolite type ZSM-5; and (v) прокаливания обработанного кислотой материала на основе цеолита типа ZSM-5 при температуре в диапазоне от приблизительно 400°С до приблизительно 600°С в течение периода времени в диапазоне от приблизительно 2 часов до приблизительно 6 часов с получением продукта на основе обескремненного цеолита типа ZSM-5 с мольным отношением диоксида кремния к оксиду алюминия от приблизительно 30 до приблизительно 80 и с площадью поверхности мезопор в диапазоне от приблизительно 150 м2/грамм до приблизительно 300 м2/грамм.(v) calcining an acid-treated ZSM-5 type zeolite material at a temperature in the range of from about 400 ° C to about 600 ° C for a period of time in the range of from about 2 hours to about 6 hours to obtain a product based on silica-free zeolite like ZSM-5 with a molar ratio of silica to alumina of from about 30 to about 80 and with a mesopore surface area in the range of from about 150 m 2 / gram to about 300 m 2 / gram. 8. Продукт на основе обескремненного цеолита типа ZSM-5 с мольным отношением диоксида кремния к оксиду алюминия от приблизительно 20 до приблизительно 150 и с площадью поверхности мезопор в диапазоне от приблизительно 100 м2/грамм до приблизительно 400 м2/грамм.8. A product based on silica-free zeolite type ZSM-5 with a molar ratio of silica to alumina of from about 20 to about 150 and with a mesopore surface area in the range of from about 100 m 2 / gram to about 400 m 2 / gram. 9. Продукт по п. 8, дополнительно содержащий носитель, выбранный из группы, состоящей главным образом из носителя из оксида алюминия, носителя из диоксида кремния, носителя из диоксида кремния-оксида алюминия, носителя из диоксида титана и носителя из диоксида циркония или любой их комбинации.9. The product of claim 8, further comprising a carrier selected from the group consisting mainly of a carrier of alumina, a carrier of silica, a carrier of silica-alumina, a carrier of titanium dioxide and a carrier of zirconia or any combinations. 10. Продукт по п. 9, дополнительно содержащий гидрирующий металл из группы, состоящей главным образом из молибдена, платины, палладия, родия, рутения, никеля, железа, осмия, иридия, вольфрама и рения.10. The product of claim 9, further comprising a hydrogenating metal from the group consisting mainly of molybdenum, platinum, palladium, rhodium, ruthenium, nickel, iron, osmium, iridium, tungsten and rhenium.
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